Process for removing nicotine from tobacco to any desired extent without destroying its aroma



May 29, 1928. 1,671,259

T. SCHLOESING PROCESS FOR nmovme NIGOTINE FROM TOBACCO TO ANY DESIRED EXTENT WITHOUT DESTROYING ITS AROMA Filed Jan. 26, 1925 A MMONIA WQTER (MLMMW W w W 2563 x been passed over (5 Patented May 29, 1928.

PATENT OFFICE.

THEOI'EILE BCHLOESING, OI PARIS, FRANCE.

PROCESS FOR REMOVING NICO'IINE FROM TOBACCO TO ANY DESIRED EXTENT WITH- OUI. DESTROYING ITS AROMA.

Application filed January 26, 1925, Serial No. 4,987, and in France May 30, 1924.

This invention relates to a process for removing nicotine from tobacco to any desired extent without destroying its aroma.

It is known that ammonia displaces nicotine and that steam can carry off nicotine vapour.

' The said process makes use of these facts but in a new'method justifying both theory and practice. It has already been proposed to remove nicotine from. tobacco by moistening the to bacco with ammonia and afterwards subject-ing it to the action of steam.

It has also been proposed to employ steam at a pressure lower than atmospheric, that is to say, a temperature below 100, with a view to decreasing the loss of the aromatic constituents in the tobacco.

Experiments have shown that if the tobacco to be treated is moistened with a solution of ammonia prior to its being subjected to. the action of steam, the nicotine canonly be removed by the steam to a certain degree and this is true even when a large amount of the ammoniacal solution is employed. This can be explained theoretically and verified by experiment. When steam is passed over tobacco treated with an ammoniacal solution, the treated tobacco carries to start with free ammonia in excess. There remains present in the tobacco ammonia salts and nicotine. There is a reciprocal displacement of ammonia and nicotine; the nicotine decomposes in part the ammonia salts, freeing the ammonia with the formation of nicotine salts and in consequence there is in the tobacco in the form of salts a certain proportion of nicotine which is not driven off by the steam. This propor; tion is substantial. It may easily be ofthe order of or 4.0% even when with the ob ject of reducing is a great deal of steam has to 10 times the weight of the tobacco). Even if the tobacco is treated with fresh additions of ammonia, it is not possible to remove all of the nicotine without prolonged action and in order to accurately determine the condition of the treated tobacco, it is necessary not only to ascertain if appreciable'quantities of alkaloid' are no longer evolved,bnt also to ascertain directly the quantity of nicotine, in the treated tobacco. V

On the other hand, according to experimental results the more steam is cm the more the tobacco is dep matic constituents, comprising under this term the various substances more or less Volatile which contributeto its taste and aroma; if only to avoid this dan er the ployed,

rived of its aros.

quantity of steam used must be restricted as preciable ammoniacal pressure is maintained 1n the medium during the whole treatment by apermanent adjunction of gaseous ammonia) which prevents the formation of nonvolatile nicotine salts and suppresses an limit to the elimination of the alkaloid: Nicotine is constantly displaced by the ammonia and carried off by the steam as. it is set free. The elimination -of the nicotine from the tobacco may be' considerable and if really desired may be complete; it may be carried out to any degree that is desired according to the quantity of steam mixed with the ammoniathat is passed over.

It has been found that if the gaseous ammonia is maintained at a proportion of a certain order when mixed with steam the elimination of the nicotine from the tobacco only depends on the quantity of ,steam employed. This suitable proportion of gaseous ammonia may be varied between wlde limits, for example, between 25 grams or even less and 160 grams oreven more of gaseous ammonia to 1 kilogram ofsteam. It is this circumstance which gives great flexibility to the rocess. It is not necessary to regulate with care and exactness the proportion of gaseous ammonia in the steam. The steam passed over has only tobe measured by condensing it and by ascertainmg the volumeof water resulting from the Q condensation, and a practical measurement mentioned above the aroma in the tobacco.

the action. It is necessar quantity of steam much less than that which must be employed, if apermanent ammoniacal pressure is not maintained.

With thismoderate use of steam there only results a very small loss of flavour and- It is so small that it is not necessary to seek to restrict it in order to keep the temperature of the operation down, so that the treatment with the steam and ammonia may be carried out at atmospheric pressure at 100 (3.; it is much more simple in operation and in the apparatus used than to operate at a lower temperature under reduced pressure.

Another method may be employed to re duce the loss of flavour to an insign' cant extent. This consists in recovering the major portion of the small quantities of aromatic constituents which have been separated from the treated materials and adding them to the mixture of steam and ammonia which is again passed over the tobacco. .After pasing over is condensed in the nicotine,

tities of aromatic constituents driven ofi. The liquor produced by condensation is thus a, solution of ammonia and nicotine conthe tobacco, the steam condenser D with the.

taining small quantities of aromatic constituents. It arrives in a container A where by means of a pipe 3 with upwardly directlaced in intimate contact as petroleum which entirely absorbs the nicotine. The ammoniacal solution being heavier than the solution occupies the bottom of the container and passes out therefrom through pipe 2 together with the aromatic constituents. The solvent in the upper part of the container passes out through pipe 1 to a container B where it is completely freed from its'dis solved nicotine by utting it in contact with an acid such as suiphuriqand then returns to A to be charged afresh with nicotine; it circulates continually from A to B and from B to A. From B is extracted the nicotine salt (sulphate for example) formed, separated from the solvent; I But the ammonia being slightly soluble in the petroleum, the steam condensate abondons to the petroleum together with nicotine, a little ammonia and there is obtained in B, owing to the action of the sulphuric acid on the petroleum coning openings it isw1th a solvent suc taining nicotine and a little ammonia, not.

only nicotine sulphate but ammonium sulphate. This latter is almost insoluble in the concentrated solution of nicotine sulphate which is formed, and atthe end of a certain time it causes the solution to become pasty, thus producing an appreciable hindrance in to free the petroleum or other solvent. 0

which solvent has beensnsed to.....cover .the

the ammonia and the small quan-,

passes out as a salt, for example, a

duces any irritation of ammonia that it contains by a method hereinafter described;

be passed into apparatus such as a plate distiller where it flows in an opposite direction to the steam, giving up all its ammonia to the steam and at the same time its aromatic constituents; it passes out as water free from ammonia.

A mixture of steam and gasous ammonia and aromatic constituents is again formed and again used to treat the tobacco. The latter should naturally be protected against cooling so that condensation in the parts in contact with the walls isavoided; this may be achieved, for example, by making the steam pass, before coming into contact with the tobacco, between the container containing the materials and a casing coated externally with nonheat-conducting material. The tobacco is ready for common use when removed from the container.

It should be remarked that it is necessary that the nicotine should be removed from the ammoniacal solution coming frpm A and entering C. If nicotine remains in this solution, it goes out of C with the steam and the gaseous ammonia; a mixture of steam and gaseous ammonia containing nicotine vapour would then be made to pass over the tobacco and then only a partial removal of the nicotine from the tobacco could be obtained, a feeble pressure of nicotine vapour preventing the removalof .this alkaloid; frequently the tobacco would be -enriched in nicotine. I

The gaseous ammonia follows a closed cycle: container C (a boiler or distiller), tobacco container R, condenser D, container where the ammonia separates from the nicotine, container C, etc. The aromatic concompensate the lossesin 'gasstituents accomp ny the gaseous ammoma.

The tobacco only ammonia.

The nicotine extracted fixes small quantities of sulphate, and constitutes a "aluable by-product.

The tobacco after treatment is milder but still contains its aroma. It no longer prothe throat and may be used without inconvenience by persons on. whom the action of nicotine is imurious.

It has been stated above that it is necessary before removing the solvent from remove any ammonia dissolved in it.

Various processes can be utilized to effect this elimination of ammonia contained in the solvent. One means consists in passing the from the tobacco v Ato solvent upwards through water, preferably in more/or less small streams or bubbles. If

the co tact of the two liquids is suflicient,

the ater retains all the ammonia with a little nicotine. This Washing water maybe re eWed gradually by making it circulate if the opposite direction to the petroleum in I such a manner'that'the lat-teris found completely deprived of its ammonia. Y. If the Water carries with it an appreciable quantity of nicotine, it can be made to enter into the cycle of operations above described.

In this process of eliminating the ammonia the water may be saturated with a salt such assodium chloride for example;

such a liquid has the advantage of dissolv-' ing less nicotine than pure water, while disso ving the ammonia nearly as well.

- Another method which is very s1mple and particularly good for the removal of the ammonia from the petroleum (or other nicotine.

and-ammonia solvent) consists in bringing the petroleum in intimate contact with gas such as air; for example, the gas could be caused to bubble into the petroleum, or the petroleum could be brought to a finely divided state by causing it to fall in thin sheets or little drops. As hereshown, the etroleum enters a purifying device E an is caused to flow over solid materials of regular or irregular shape, for instance, pebbles or the like, and a current of air is caused to" pass over the petrol thus divided. The current of'air would take with it very readily all the ammonia without taking ofi at the same timean appreciable quantity of nicetine vapour. The ammonia led off by the gaseous current is easily recovered byany known means, for example, by passing the gaseous current in a container where it is put into contact with an acid.

What I claim is: V 1. A process for removing nicotine fro tobacco without destroying the aroma of the latter, which consists in circulating a mixture of steam and gaseous ammonia through the tobacco in a closed system, removing the entrained nicotine from said mixture, and

again passing the mixture over the tobacco.

2. A process for removing nicotine from tobacco, consisting in treating tobacco. with a mixture of steam and gaseous ammonia,

condensing said mixture, removing the nico-' tine from saidcondensate by meansof a solvent, recovering the nicotine from said solvent, vaporizing said condensate, and reintroducing sald vaporized condensate and said solvent in the cycle ofoperatlons.

3. A process for removing nicotine from tobacco, consisting, in treating tobacco with a mixture of steam and gaseous ammonia, condensing said mixture,'removing the nicotine from said condensate by means of a solvent, recovering the nicotine from said solvent, removing the ammonia from said solvent, vaporizing saidcondensate and reintroducing said vaporized condensate and said,

sate, and reintroducing said vaporized condensate and said solvent in the cycle of perations. i

5. A process for removing nicotine frm tobacco without destroying the aroma of the latter, which consists in circulating a mixture ofsteam and gaseous ammonia through the tobacco, the proportion of ammonia gas in the mixture being substantially 25 grams to one'kilo ram of steam, removing the nicotine from the mixture, and again passing the mixture over the tobacco.

6. A process for removing tobacco without destroying t nicotine from e aroma of the latter, Which-includes circulating a 'mixture of steam and gaseous ammonia through the tobacco, entrainingthe removed nicotine in petroleum and returning the ammonia gas, steam and aromatic constituents to the tobacco. r

7. A process for remov 1n nicotine from tobacco without'destroying t e aroma of the latter, which includes the steps of passing a mixture of steam and gaseous ammonia through the tobacco, introducing this mixture with the constituents removed from the tobacco into petroleum, drawing off the petroleu'm and nicotine, removing the nicotine from the petroleum, purifying the petroleum, and returnin the same to a circuit in which the steam an ammonia gas circulate.

THE-OPH'ILE scHLoEsING. 

